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Keywords = raman microscopy

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14 pages, 5321 KB  
Article
Facile Low-Temperature Deposition of Seedless Nanocrystalline Diamond Films from CH4/Ar Gas Mixtures
by Luis Medina-Zazueta, Frank Romo-García, Miguel Martínez-Gil, Rolando Flores-Ochoa, Mathías Martinez-Gil, Dainet Berman-Mendoza, Antonio Ramos-Carrazco, Gerardo Valenzuela-Hernández, Ch. J. Salas-Juárez, Carlos A. Pérez-Rábago and Rafael García-Gutiérrez
Crystals 2026, 16(1), 10; https://doi.org/10.3390/cryst16010010 - 24 Dec 2025
Abstract
Nanocrystalline diamond (NCD) films were synthesized by microwave plasma chemical vapor deposition (MPCVD) from a CH4/Ar mixture on seedless p-type Si(111) substrates at 100–400 °C. Crystallinity was evaluated by X-ray diffraction (Cu Kα); bonding by Raman spectroscopy and X-ray photoelectron spectroscopy [...] Read more.
Nanocrystalline diamond (NCD) films were synthesized by microwave plasma chemical vapor deposition (MPCVD) from a CH4/Ar mixture on seedless p-type Si(111) substrates at 100–400 °C. Crystallinity was evaluated by X-ray diffraction (Cu Kα); bonding by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS); morphology and thickness by scanning electron microscopy (SEM); defect states by thermoluminescence (TL). SEM shows continuous films with uniform thickness. XRD displays a broad (111) reflection near 2θ = 44°. Raman and XPS reveal temperature-dependent bonding: between 300 and 400 °C, the sp3 fraction increases relative to sp2. TL glow curves show peaks at 157 °C and 270 °C, indicating electron-trap centers. These results demonstrate hydrogen-free and seedless NCD growth at low substrate temperatures, supporting potential electronic and dosimetry applications requiring a low thermal load. Full article
(This article belongs to the Special Issue Advances in Thin-Film Materials and Their Applications)
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24 pages, 4792 KB  
Article
Modification of Physico-Chemical and Biological Characteristics of Polymethylmethacrylate with Amorphous Carbon Nanoparticles for Counteracting Healthcare-Associated Infections
by Sergey V. Gudkov, Dmitriy A. Serov, Ruslan M. Sarimov, Vasiliy S. Novikov, Maksim Moskovskiy, Maksim B. Rebezov, Mikhail V. Dubinin, Konstantin V. Sergienko, Mikhail A. Sevostyanov, Fatikh M. Yanbaev, Maxim E. Astashev and Maria V. Vedunova
J. Funct. Biomater. 2026, 17(1), 5; https://doi.org/10.3390/jfb17010005 - 21 Dec 2025
Viewed by 160
Abstract
Composite materials based on polymethylmethacrylate (PMMA) and carbon nanoparticles are used in aviation, construction, medical and other fields of activity. Carbon nanotubes and carbon nano-dots are mainly used as carbon nanoparticles. Both carbon nanotube and carbon nano-dots are difficult to obtain materials with [...] Read more.
Composite materials based on polymethylmethacrylate (PMMA) and carbon nanoparticles are used in aviation, construction, medical and other fields of activity. Carbon nanotubes and carbon nano-dots are mainly used as carbon nanoparticles. Both carbon nanotube and carbon nano-dots are difficult to obtain materials with considerable cost. Amorphous carbon nanoparticles, on the contrary, are easy to obtain and have a low cost. The purpose of this work is to study the physico-chemical and biological characteristics of polymethylmethacrylate modified with amorphous carbon nanoparticles. Laser ablation was used to obtain the nanoparticles. Dynamic light scattering, measurement of the electrokinetic potential, TEM, AFM, and Raman microscopy are used to characterize nanoparticles. FTIR, MIM, AFM, UV-visual diagnostics, ROS tests, and biopolymer regeneration tests were used to analyze the combined sensors. The bacteriostatic effect was evaluated using turbodimetry, and the antibacterial effect was evaluated using precision cytofluorometry. Mammalian cells were examined using fluorescence microscopy. Carbon nanoparticles (CNPs) have been obtained and characterized. A protocol has been developed for the introduction of CNPs into photolithographic resin. Printed samples of complex geometry. It is shown that the printed samples are amenable to polishing, have pro-oxidant properties, and are able to prevent damage to biopolymers. Printed samples inhibit the development of bacteria and cause loss of viability. At the same time, the printed samples do not affect the development of mammalian cells. The obtained resins based on PMMA with CNPs can potentially serve as the basis for the creation of non-toxic materials in biomedicine and pharmacology. Full article
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21 pages, 3790 KB  
Article
Surface Engineering of PET Fabrics with TiO2 Nanoparticles for Enhanced Antibacterial and Thermal Properties in Medical Textiles
by Muhammad Zaman Khan, Azam Ali, Hadi Taghavian, Jakub Wiener, Jiri Militky and Dana Křemenáková
Textiles 2025, 5(4), 71; https://doi.org/10.3390/textiles5040071 - 18 Dec 2025
Viewed by 131
Abstract
Medical textiles have gained significant attention for their ability to prevent the transmission of infectious diseases while ensuring the safety and comfort of healthcare professionals. This study focuses on modifying the surfaces of polyethylene terephthalate (PET) fabrics with titanium dioxide (TiO2) [...] Read more.
Medical textiles have gained significant attention for their ability to prevent the transmission of infectious diseases while ensuring the safety and comfort of healthcare professionals. This study focuses on modifying the surfaces of polyethylene terephthalate (PET) fabrics with titanium dioxide (TiO2) nanoparticles (NPs) to enhance their antibacterial properties, thermophysiological comfort, and thermal insulation. The effects of varying volumes of the tetraisopropyl orthotitanate precursor on the functional properties of the coated PET fabrics were systematically investigated. The surface morphology was characterized using scanning electron microscopy (SEM). At the same time, the elemental and chemical properties were analyzed through Energy-dispersive spectroscopy (EDS), Raman spectroscopy, and Fourier-transform infrared spectroscopy (FTIR). The TiO2 NPs-coated PET fabrics demonstrated exceptional antibacterial activity against Gram-negative and Gram-positive bacteria and significantly improved thermophysiological comfort. Specifically, thermal resistance increased with a higher density of TiO2 nanoparticles, leading to a decrease in thermal conductivity. Notably, only minimal reductions were observed in relative water vapor permeability (RWVP) and air permeability (AP), indicating that the fabric’s porosity was maintained. Furthermore, the presence of the TiO2 nanolayer on the PET fabric significantly enhanced its thermal stability, providing excellent thermal insulation properties. These findings underscore the potential of TiO2 NPs-coated PET fabrics as promising candidates for advanced medical textile applications, where a balance of protection, comfort, and thermal insulation is essential. Full article
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14 pages, 6934 KB  
Article
Characterization and Analysis of Gypsum Alabaster Constituting the “Santissimo Salvatore” Statue by Gabriele Brunelli (Bologna, 1615–1682)
by Camilla Favale, Gianfranco Ulian, Gian Carlo Grillini, Daniele Moro and Giovanni Valdrè
Heritage 2025, 8(12), 543; https://doi.org/10.3390/heritage8120543 - 17 Dec 2025
Viewed by 135
Abstract
This study is part of a broader conservation and restoration project of the 17th-century statue “Santissimo Salvatore” attributed to the Bolognese sculptor Gabriele Brunelli (1615–1682). This sculpture was traditionally classified as a marble statue, i.e., primarily composed of calcium carbonate. However, [...] Read more.
This study is part of a broader conservation and restoration project of the 17th-century statue “Santissimo Salvatore” attributed to the Bolognese sculptor Gabriele Brunelli (1615–1682). This sculpture was traditionally classified as a marble statue, i.e., primarily composed of calcium carbonate. However, the careful diagnostic analyses conducted during the present work of restoration revealed that, instead, the sculpture is made of gypsum alabaster, a material predominantly composed of calcium sulphate hydrate (CaSO4·2H2O). In the present research, a multi-analytical investigation was carried out using X-Ray Powder Diffraction (XRPD), Field Emission Environmental Scanning Electron Microscopy (FE-ESEM) with Energy-Dispersive X-ray Spectroscopy (EDS), and confocal Raman microspectrometry. Here, we report detailed and updated analytical data of the material constituting the “Santissimo Salvatore” statue by Gabriele Brunelli. These data were found extremely useful to plan and accomplish the restoration work in detail: (i) the suitable conservation project of the artwork, (ii) the reassessment of the knowledge on the artist’s sculptural production, and (iii) gaining more information about the material used in the 17th-century Bolognese sculptural context. Full article
(This article belongs to the Section Cultural Heritage)
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29 pages, 18594 KB  
Article
Weathering and Restoration of Traditional Rammed-Earth Walls in Fujian, China
by Carlos Ka Nok Lo and Junxin Song
Coatings 2025, 15(12), 1491; https://doi.org/10.3390/coatings15121491 - 17 Dec 2025
Viewed by 153
Abstract
Traditional rammed-earth buildings, a key component of Fujian’s architectural heritage, are increasingly vulnerable to environmental degradation and urban relocation. This study focuses on the weathering patterns and restoration strategies of the rammed-earth walls at Zishantang, a typical 19th-century residence in Yongtai County. Through [...] Read more.
Traditional rammed-earth buildings, a key component of Fujian’s architectural heritage, are increasingly vulnerable to environmental degradation and urban relocation. This study focuses on the weathering patterns and restoration strategies of the rammed-earth walls at Zishantang, a typical 19th-century residence in Yongtai County. Through SEM, EDS, XRD, and Raman spectroscopy, eight groups of samples were analyzed to evaluate microstructural deterioration under different forms of environmental exposure. Results show that walls lacking intact soot ash coatings (“Wu-yan-hui”) exhibit greater porosity, microcracking, and mineral loss—particularly on exposed facades. These findings highlight the protective role of traditional soot–lime coatings and suggest that orientation and exposure-specific conservation strategies are essential. This study provides a scientific basis for preserving the material authenticity and structural integrity of relocated rammed-earth heritage in humid subtropical climates. Full article
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14 pages, 1343 KB  
Article
Research on the Formation Mechanisms of Red Stains on Outdoor Marble Cultural Relics at Beijing Confucian Temple and the Imperial College
by Yuanyuan Wang, Jiaru Liu, Yi Zhou, Wenjia Hu, Jiao Pan and Jianrui Zha
Coatings 2025, 15(12), 1488; https://doi.org/10.3390/coatings15121488 - 17 Dec 2025
Viewed by 159
Abstract
Stone relics exposed to outdoor environments frequently experience surface deterioration, with red stains being a common and persistent issue. The stains often observed on marble and limestone surfaces arise from complex interactions involving chemical reaction, pollutant deposition, and microbiological process. Although microbial colonization [...] Read more.
Stone relics exposed to outdoor environments frequently experience surface deterioration, with red stains being a common and persistent issue. The stains often observed on marble and limestone surfaces arise from complex interactions involving chemical reaction, pollutant deposition, and microbiological process. Although microbial colonization has been associated with biodeterioration, the specific mechanisms remain poorly understood. This study focuses on the red stains found on the Danbi marble carvings at Beijing Confucian Temple and the Imperial College. Combining microbial cultivation, molecular identification (ITS sequencing), SEM-EDS (Scanning Electron Microscopy), Raman spectroscopy, and HPLC-MS (high-performance liquid chromatography with mass spectrometry), we identified the pigment-producing fungus Lizonia empirigonia as the dominant agent, with no evidence of inorganic contributors such as iron/lead oxides. Metabolite profiling revealed flavonoids and polyketides as key coloring material, while controlled infection experiments demonstrated the fungus’s reliance on exogenous organic matter rather than direct stone degradation. Our findings highlight microbial activity as a primary driver of red stains in marble relics and underscore the importance of organic contaminant control in conservation. Full article
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16 pages, 5931 KB  
Article
Deposition and Properties of Nanostructured Multilayer Cr/(Cr/a-C)ml Coating on Stainless Steels
by Valentin Mishev, Yavor Sofronov, Milko Yordanov, Antonio Nikolov, Krum Petrov, Rayna Dimitrova, Milko Angelov, Boyan Dochev, Krassimir Marchev and Georgi Todorov
Materials 2025, 18(24), 5654; https://doi.org/10.3390/ma18245654 - 16 Dec 2025
Viewed by 109
Abstract
This work presents the results of deposition by magnetron sputtering nanostructured multilayer Cr/(Cr/a-C)ml coatings on AISI 316L and AISI 321 steel substrates. Chemical compositions were confirmed through EDX analysis with scanning electron microscopy. The coating thickness was measured with Calotester (KaloMAX II) and [...] Read more.
This work presents the results of deposition by magnetron sputtering nanostructured multilayer Cr/(Cr/a-C)ml coatings on AISI 316L and AISI 321 steel substrates. Chemical compositions were confirmed through EDX analysis with scanning electron microscopy. The coating thickness was measured with Calotester (KaloMAX II) and the total thickness of the coatings obtained ranged from 1.684 ± 0.193 μm for AISI 316L to 1.749 ± 0.123 μm for AISI 321. A Daimler-Benz Rockwell indentation test for adhesion quality and a nanoindentation test with a Berkovich indenter were carried out. According to the Raman spectroscopy analysis and in agreement with mechanical tests, it is supposed that it is the formation of a diamond-like carbon phase which enhances the mechanical properties. The hardness values obtained for the nanostructured multilayer Cr/(Cr/a-C)ml coatings were improved compared to those of the base stainless steels. Full article
(This article belongs to the Special Issue Micro/Nano-Structured Material Surfaces and Their Functional Coatings)
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20 pages, 19282 KB  
Article
Single-Exosome SERS Detection by Means of a Flexible Metasurface
by Konstantin Mochalov, Denis Korzhov, Milena Shestopalova, Andrey Ivanov, Konstantin Afanasev, Alexander Smyk, Alexander Shurygin and Andrey K. Sarychev
Biosensors 2025, 15(12), 815; https://doi.org/10.3390/bios15120815 - 15 Dec 2025
Viewed by 348
Abstract
Single exosomes are detected via surface-enhanced Raman scattering (SERS) due to electromagnetic field accumulation on a specially designed flexible metasurface. This metasurface is a modulated silver nanofilm deposited on a thin, flexible plastic substrate. An explicit Equation for calculating the local electric field [...] Read more.
Single exosomes are detected via surface-enhanced Raman scattering (SERS) due to electromagnetic field accumulation on a specially designed flexible metasurface. This metasurface is a modulated silver nanofilm deposited on a thin, flexible plastic substrate. An explicit Equation for calculating the local electric field is given. The field reaches extremely high values under plasmon resonance conditions and fills the depressions of the metasurface. The thin, flexible metasurface can be incorporated into automated Lab-On-Chip analytical systems and used for spectroscopic studies of exosomes. We propose a method to distinguish individual exosomes from the HEK293T cell line on the metasurface and then obtain and assign their SERS spectra. An important advantage of the plasmonic metasurface presented in this work is its spatial complementarity to exosomes and other vesicle-like objects. The plasmonic metasurface is fabricated using holographic lithography and further investigated using a correlation approach combining atomic force microscopy, scanning spreading resistance microscopy, and surface-enhanced spectroscopy. Full article
(This article belongs to the Special Issue Raman Scattering-Based Biosensing)
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22 pages, 6432 KB  
Article
Minerals as Windows into Habitability on Lava Tube Basalts: A Biogeochemical Study at Lava Beds National Monument, CA
by Dina M. Bower, Amy C. McAdam, Clayton S. C. Yang, Feng Jin, Maeva Millan, Clara Christiann, Mathilde Mussetta, Christine Knudson, Jamielyn Jarvis, Sarah Johnson, Zachariah John, Catherine Maggiori, Patrick Whelley and Jacob Richardson
Minerals 2025, 15(12), 1303; https://doi.org/10.3390/min15121303 - 14 Dec 2025
Viewed by 254
Abstract
Lava tubes on Earth provide unique hydrogeological niches for life to proliferate. Orbital observations of the Martian surface indicate the presence of lava tubes, which could hold the potential for extant life or the preservation of past life within a subsurface environment protected [...] Read more.
Lava tubes on Earth provide unique hydrogeological niches for life to proliferate. Orbital observations of the Martian surface indicate the presence of lava tubes, which could hold the potential for extant life or the preservation of past life within a subsurface environment protected from harsh conditions or weathering at the surface. Secondary minerals in lava tubes form as a combination of abiotic and biotic processes. Microbes colonize the surfaces rich in these secondary minerals, and their actions induce further alteration of the mineral deposits and host basalts. We conducted a biogeochemical investigation of basaltic lava tubes in the Medicine Lake region of northern California by characterizing the compositional variations in secondary minerals, organic compounds, microbial communities, and the host rocks to better understand how their biogeochemical signatures could indicate habitability. We used methods applicable to landed Mars missions, including Raman spectroscopy, X-ray diffraction (XRD), Laser-Induced Breakdown Spectroscopy (LIBS), and gas chromatography–mass spectrometry (GC-MS), along with scanning electron microscopy (SEM) and metagenomic DNA/RNA sequencing. The main secondary minerals, amorphous silicates, and calcite, formed abiotically from the cave waters. Two types of gypsum, large euhedral grains with halites, and cryptocrystalline masses near microbial material, were observed in our samples, indicating different formation pathways. The cryptocrystalline gypsum, along with clay minerals, was associated with microbial materials and biomolecular signatures among weathered primary basalt minerals, suggesting that their formation was related to biologic processes. Some of the genes and pathways observed indicated a mix of metabolisms, including those involved in sulfur and nitrogen cycling. The spatial relationships of microbial material, Cu-enriched hematite in the host basalts, and genetic signatures indicative of metal cycling also pointed to localized Fe oxidation and mobilization of Cu by the microbial communities. Collectively these results affirm the availability of bio-essential elements supporting diverse microbial populations on lava tube basalts. Further work exploring these relationships in lava tubes is needed to unravel the intertwined nature of abiotic and biotic interactions and how that affects habitability in these environments on Earth and the potential for life on Mars. Full article
(This article belongs to the Special Issue Exploring Novel Interactions Between Microbes and Minerals)
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25 pages, 4782 KB  
Article
Comprehensive Structural and Interfacial Characterization of Laser-Sliced SiC Wafers
by Hong Chen, Seul Lee, Minseung Kang, Hye Seon Youn, Seongwon Go, Eunsook Kang and Chae-Ryong Cho
Materials 2025, 18(24), 5615; https://doi.org/10.3390/ma18245615 - 14 Dec 2025
Viewed by 362
Abstract
Laser slicing has emerged as a promising low-kerf and low-damage technique for SiC wafer fabrication; however, its effects on the crystal integrity, near-surface modification, and charge-transport properties require further clarification. Here, a heavily N-doped 4° off-axis 4H-SiC wafer was sliced using an ultraviolet [...] Read more.
Laser slicing has emerged as a promising low-kerf and low-damage technique for SiC wafer fabrication; however, its effects on the crystal integrity, near-surface modification, and charge-transport properties require further clarification. Here, a heavily N-doped 4° off-axis 4H-SiC wafer was sliced using an ultraviolet (UV) picosecond laser, and both laser-irradiated and laser-sliced surfaces were comprehensively characterized. X-ray diffraction and pole figure measurements confirmed that the 4H stacking sequence and macroscopic crystal orientation were preserved after slicing. Raman spectroscopy, including analysis of the folded transverse-optical and longitudinal-optical phonon–plasmon coupled modes, enabled dielectric function fitting and determination of the plasmon frequency, yielding a free-carrier concentration of ~3.1 × 1018 cm−3. Hall measurements provided consistent carrier density, mobility, and resistivity, demonstrating that the laser slicing process did not degrade bulk electrical properties. Multi-scale Atomic Force Microscopy (AFM), Angle-Resolved X-Ray Photoelectron Spectroscopy (ARXPS), Secondary Ion Mass Spectrometry (SIMS), and Transmission Electron Microscopy (TEM)/Selected Area Electron Diffraction (SAED) analyses revealed the formation of a near-surface thin amorphous/polycrystalline modified layer and an oxygen-rich region, with significantly increased roughness and thicker modified layers on the hilly regions of the sliced surface. These results indicate that UV laser slicing maintains the intrinsic crystalline and electrical properties of 4H-SiC while introducing localized nanoscale surface damage that must be minimized by optimizing the slicing parameters and the subsequent surface-finishing processes. Full article
(This article belongs to the Section Advanced Materials Characterization)
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21 pages, 5803 KB  
Article
Microwave-Assisted Synthesis of Visible Light-Driven BiVO4 Nanoparticles: Effects of Eu3+ Ions on the Luminescent, Structural, and Photocatalytic Properties
by Dragana Marinković, Bojana Vasiljević, Nataša Tot, Tanja Barudžija, Sudha Maria Lis Scaria, Stefano Varas, Rossana Dell’Anna, Alessandro Chiasera, Bernhard Fickl, Bernhard C. Bayer, Giancarlo C. Righini and Maurizio Ferrari
Molecules 2025, 30(24), 4757; https://doi.org/10.3390/molecules30244757 - 12 Dec 2025
Viewed by 304
Abstract
The optimization of BiVO4-based structures significantly contributes to the development of a global system towards clean, renewable, and sustainable energies. Enhanced photocatalytic performance has been reported for numerous doped BiVO4 materials. Bi3+-based compounds can be easily doped with [...] Read more.
The optimization of BiVO4-based structures significantly contributes to the development of a global system towards clean, renewable, and sustainable energies. Enhanced photocatalytic performance has been reported for numerous doped BiVO4 materials. Bi3+-based compounds can be easily doped with rare earth (RE3+) ions due to their equal valence and similar ionic radius. This means that RE3+ ions could be regarded as active co-catalysts and dopants to enhance the photocatalytic activity of BiVO4. In this study, a simple microwave-assisted approach was used for preparing nanostructured Bi1−xEuxVO4 (x = 0, 0.03, 0.06, 0.09, and 0.12) samples. Microwave heating at 170 °C yields a bright yellow powder after 10 min of radiation. The materials are characterized through X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet–visible–near-infrared diffuse reflectance spectroscopy (UV-Vis-NIR DRS), photoluminescence spectroscopy (PL), and micro-Raman techniques. The effects of the different Eu3+ ion concentrations incorporated into the BiVO4 matrix on the formation of the monoclinic scheelite (ms-) or tetragonal zircon-type (tz-) BiVO4 structure, on the photoluminescent intensity, on the decay dynamics of europium emission, and on photocatalytic efficiency in the degradation of Rhodamine B (RhB) were studied in detail. Additionally, microwave chemistry proved to be beneficial in the synthesis of the tz-BiVO4 nanostructure and Eu3+ ion doping, leading to an enhanced luminescent and photocatalytic performance. Full article
(This article belongs to the Special Issue Chemiluminescence and Photoluminescence of Advanced Compounds)
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17 pages, 3608 KB  
Article
Mechanochemically Synthesized Nanocrystalline Cu2ZnSnSe4 as a Multifunctional Material for Energy Conversion and Storage Applications
by Angel Agnes Johnrose, Devika Rajan Sajitha, Vengatesh Panneerselvam, Anandhi Sivaramalingam, Kamalan Kirubaharan Amirtharaj Mosas, Beauno Stephen and Shyju Thankaraj Salammal
Nanomaterials 2025, 15(24), 1866; https://doi.org/10.3390/nano15241866 - 12 Dec 2025
Viewed by 301
Abstract
Cu2ZnSnSe4 is a promising light-absorbing material for cost-effective and eco-friendly thin-film solar cells; however, its synthesis often leads to secondary phases that limit device efficiency. To overcome these challenges, we devised a straightforward and efficient method to obtain single-phase Cu [...] Read more.
Cu2ZnSnSe4 is a promising light-absorbing material for cost-effective and eco-friendly thin-film solar cells; however, its synthesis often leads to secondary phases that limit device efficiency. To overcome these challenges, we devised a straightforward and efficient method to obtain single-phase Cu2ZnSnSe4 nanocrystalline powders directly from the elements Cu, Zn, Sn, and Se via mechanochemical synthesis followed by vacuum annealing at 450 °C. Phase evolution monitored by X-ray diffraction (XRD) and Raman spectroscopy at two-hour milling intervals confirmed the formation of phase-pure kesterite Cu2ZnSnSe4 and enabled tracking of transient secondary phases. Raman spectra revealed the characteristic A1 vibrational modes of the kesterite structure, while XRD peaks and Rietveld refinement (χ2 ~ 1) validated single-phase formation with crystallite sizes of 10–15 nm and dislocation densities of 3.00–3.20 1015 lines/m2. Optical analysis showed a direct bandgap of ~1.1 eV, and estimated linear and nonlinear optical constants validate its potential for photovoltaic applications. Scanning electron microscopy (SEM) analysis showed uniformly distributed particles 50–60 nm, and energy dispersive X-ray (EDS) analysis confirmed a near-stoichiometric Cu:Zn:Sn:Se ratio of 2:1:1:4. X-ray photoelectron spectroscopy (XPS) identified the expected oxidation states (Cu+, Zn2+, Sn4+, and Se2−). Electrical characterization revealed p-type conductivity with a mobility (μ) of 2.09 cm2/Vs, sheet resistance (ρ) of 4.87 Ω cm, and carrier concentrations of 1.23 × 1019 cm−3. Galvanostatic charge–discharge testing (GCD) demonstrated an energy density of 2.872 Wh/kg−1 and a power density of 1083 W kg−1, highlighting the material’s additional potential for energy storage applications. Full article
(This article belongs to the Section Energy and Catalysis)
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21 pages, 4961 KB  
Article
Toward a Correlative Metrology Approach on the Same 2D Flake: Graphene Oxide Case Study—Sample Preparation and Stability Issues
by Lydia Chibane, Alexandra Delvallée, Nolwenn Fleurence, Sarah Douri, José Morán-Meza, Christian Ulysse, François Piquemal, Nicolas Feltin and Emmanuel Flahaut
Nanomaterials 2025, 15(24), 1861; https://doi.org/10.3390/nano15241861 - 11 Dec 2025
Viewed by 232
Abstract
Although graphene promises a wide range of applications, large-scale production of this material remains complex. One very common way of obtaining graphene is through a reduction in graphene oxide (GO). In order to fully control this production process, it is necessary to obtain [...] Read more.
Although graphene promises a wide range of applications, large-scale production of this material remains complex. One very common way of obtaining graphene is through a reduction in graphene oxide (GO). In order to fully control this production process, it is necessary to obtain data from different techniques, but a comprehensive characterization methodology and associated metrology are currently lacking. Here, we propose tools for substrate selection (in this study, the most appropriate were silicon and silicon dioxide on silicon) and precautions to be taken when setting up a correlative metrology method integrating atomic force microscopy (AFM), scanning electron microscopy (SEM), Raman microscopy/spectroscopy, scanning microwave microscopy (SMM) and scanning thermal microscopy (SThM). Indeed, in order to obtain reliable data for each of these techniques applied to a unique graphene oxide flake, a strategy must be developed and could be implemented to monitor the reduction in GO. Emphasis was placed on the choice of the substrate and on the possible degradations generated by each of the techniques employed, and a running sequence was determined. Full article
(This article belongs to the Special Issue A Sustainable Future Using 2D and 1D Nanomaterials and Nanotechnology)
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13 pages, 2897 KB  
Article
A Mild Iodide–Triiodide Redox Pathway for Alkali-Metal and Ammonium Ion Intercalation into Layered Tungsten Oxychloride (WO2Cl2)
by John Samuel, Jefferson Carter, John Ackerman, Jinke Tang and Brian Leonard
Inorganics 2025, 13(12), 403; https://doi.org/10.3390/inorganics13120403 - 11 Dec 2025
Viewed by 256
Abstract
A novel and facile route for intercalating alkali-metal ions and ammonium ions into the layered mixed-ion compound tungsten oxychloride (WO2Cl2) has been developed using the iodide–triiodide redox couple as a mild redox-active reagent. Unlike traditional intercalation techniques employing highly [...] Read more.
A novel and facile route for intercalating alkali-metal ions and ammonium ions into the layered mixed-ion compound tungsten oxychloride (WO2Cl2) has been developed using the iodide–triiodide redox couple as a mild redox-active reagent. Unlike traditional intercalation techniques employing highly reducing and air-sensitive reagents such as n-butyllithium, alkali triethylborohydride, and naphthalenide, the I/I3 redox system operates at a moderate potential (0.536 V vs. SHE), enabling safer handling under ambient conditions without stringent inert-atmosphere requirements. This redox pair promotes the reduction of W6+ to W5+, thereby facilitating cation insertion into the van der Waal (vdW) gaps of WO2Cl2. This method uniquely enables ammonium ion intercalation into WO2Cl2, a first for this system. Intercalation was confirmed by X-ray diffraction, scanning electron microscopy (SEM/EDS), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS), with measured lattice expansion correlating well with Shannon ionic radii and coordinating environments. Electrical transport measurements reveal a transition from insulating WO2Cl2 to a semiconducting phase for K0.5WO2Cl2, exhibiting a resistance drop of over four orders of magnitude. This work demonstrates the I/I3 couple as a general, safe, and versatile method for layered mixed-anion materials, broadening the chemical toolkit for low-temperature, solution-based tuning of structures and properties. Full article
(This article belongs to the Special Issue Feature Papers in Inorganic Solid-State Chemistry 2025)
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29 pages, 8639 KB  
Article
Investigation of Two Folding Screens by Futurist Artist Giacomo Balla
by Rika Pause, Madeleine Bisschoff, Suzan de Groot, Margje Leeuwestein, Saskia Smulders, Elsemieke G. van Rietschoten and Inez D. van der Werf
Heritage 2025, 8(12), 518; https://doi.org/10.3390/heritage8120518 - 10 Dec 2025
Viewed by 171
Abstract
Two folding screens by futurist artist Giacomo Balla (1871–1958) in the collection of the Kröller-Müller Museum (the Netherlands) were investigated: Paravento con linea di velocità (1916–1917) and Paravento (1916/1917–1958). The screens are painted on both sides, the first on four canvases, stretched onto [...] Read more.
Two folding screens by futurist artist Giacomo Balla (1871–1958) in the collection of the Kröller-Müller Museum (the Netherlands) were investigated: Paravento con linea di velocità (1916–1917) and Paravento (1916/1917–1958). The screens are painted on both sides, the first on four canvases, stretched onto two wooden strainers and framed with painted wooden strips, and the second on wooden panels set into four painted stiles. In the past, damages on Paravento con linea di velocità were restored by conservators, while Paravento was probably first reworked by the artist himself and later restored by conservators. Yellowed varnish and discolored retouches on both screens led to a wish for treatment. The aim of this research was to gain insight into the painting techniques, layer buildup, pigments, binders, and varnishes of the two artworks. This information supported the decision making for treatment, and it broadens the knowledge on the materials used by Balla. Up to now, only a few published studies deal with the technical examination of paintings by this artist. Both folding screens were subjected to technical photography (UV, IR photography, and X-ray) and were examined with portable point X-ray fluorescence (pXRF) and Raman spectroscopy. Moreover, samples were taken. Cross-sections were studied with optical microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX), attenuated total reflection Fourier-transform infrared (ATR-FTIR) imaging, and micro-Raman spectroscopy. Loose samples were examined with SEM-EDX, FTIR and micro-Raman spectroscopy, and pyrolysis gas chromatography mass spectrometry (Py-GC/MS). For Paravento con linea di velocità, all pigments and fillers of the painted canvases are compatible with the dating of the screen (1916–1917), but they differ from those on the frame. Here, rutile, in combination with various pigments, among which are blue copper phthalocyanine (PB15) and other synthetic organic pigments, was found. This indicates that the frame has been painted later, likely after the Second World War. The composition of the binders differs as well. Drying oil and pine resin have been used on the canvases, explaining the smooth and glossy appearance and solvent-sensitivity of the paint. On the frame, oil with some alkyd resin was identified. The provenance of the screen before 1972 is not clear, nor when the frame was made and painted and by whom. The results for Paravento indicate that the palettes of the two sides—painted in different styles—are comparable. Mainly inorganic pigments were found, except for the dark red areas, where toluidine red (PR3) is present. pXRF showed high amounts of zinc; cross-sections revealed that zinc white is present in the lower layers. These pigments are compatible with the dating of the screen (1916–1917). In many of the upper paint layers though, except for some green, dark red, and black areas, rutile has been identified. This indicates that these layers were applied later, likely after the Second World War. Since this folding screen was used by the artist and his family until his death in 1958, it seems likely that Balla himself reworked the screen. Full article
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Figure 1

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